Malaysian Journal of Chemistry

Synthesis, Characterization, and Activity Test of ZSM-5 Based on

Lapindo Mud as a Catalyst for Pyrolysis Polyethylene Plastic
Waste

Saidatul Kholidia1), Elva Arista1), Finurika Rohmati1), Jevon Febriano Soegiono1), Fatur
Rachman1), Aman Santoso1)*
1
Departmen of Chemistry, Faculty of Mathematics and Natural Science, Universitas Negeri
Malang, Indonesia
*Corresponding author (e-mail: [email protected])

Pyrolysis is potential solution to the problem of plastic waste by converting into

renewable fuel. Low-density polyethylene (LDPE) is the most common type of plastic
waste and has the potential to be pyrolyzed. A good catalyst for pyrolysis is ZSM-5,
but it’s expensive. In this research, ZSM-5 catalyst was synthesized with silica
precursor from lapindo mud without an organic template. Pyrolysis was focused on
determining the effect of variation ZSM-5 catalyst addition (0% dan 2,5%) on the
yield, quality, and chemical compound of pyrolysis liquid products. ZSM-5 catalyst
synthesized was characterized by XRF, XRD, FTIR, SEM, and surface area by
methylene blue adsorption. The silica precursor from Lapindo mud in this research
has a purity of up to 97,7% with a yield of 96,9%. ZSM-5 catalyst has been
successfully synthesized which is shown by the appearance of diffractogram peaks
that correct to ZSM-5 standard on JCPDS No. 10 235-242, hexagonal geometry, and
ZSM-5 functional group vibrational bands. The surface area of ZSM-5 in this research
is 283,94 m2/g and then used for pyrolysis reaction. The yield of liquid using a
catalyst is greater than without a catalyst. Based data on SNI 8415:2017, the resulting
liquid product has similarities to gasoline
Key words: pyrolysis; low-density polyethylene; ZSM-5; lapindo mud; gasoline.

INTRODUCTION
The use of plastic continues to increase and is massive in various sectors, even amidst
the problem of suboptimal waste management. Plastic waste ranks second in terms of the
amount of waste in Indonesia [1]. The existence of plastic waste is still a serious problem in
nationally and internationally. According to the Ministry of Environment and Forestry
(KLHK), the population of plastic waste in Indonesia is estimated to increase until 23-27
million tons by 2040. The increase of plastic waste has a dangerous impact on the
environment and global ecosystem because plastic has a long polymer chain, so it takes a
long time to degrade into a short chain. In addition, plastic waste also poses a risk to human
health through the formation of microplastics [2].
Types of plastic waste commonly found are polypropylene (PP), polyvinyl chloride
(PVC), polystyrene (PS), polyethylene terephthalate (PET), and polyethylene (PE).
Polyethylene is the most widely produced type of plastic, accounting for 48% of total plastic
production [3]. According to the Environmental Protection Agency (EPA), only 5.7% of
polyethylene plastic waste is recycled. Polyethylene plastic is a plastic composed of long and
repeating ethylene monomers. This plastic is widely used as plastic bags, food packaging,
electronic packaging, and plastic bottles in the form of low-density polyethylene (LDPE).
 Low density polyethylene (LDPE) is a type of polyethylene plastic that has branched
polyethylene chains so that the polyethylene chains are not close together. This results in
LDPE having a low density of about 0.91-0.94 g/cm 3 and being flexible [4]. The process of
processing LDPE plastic waste is mostly done by burning it conventionally. However, this
process is not effective because burning LDPE plastic actually produces gases that are
harmful to humans and pollute the air. Therefore, efforts are needed to procescatalystss
LDPE plastic waste in a more environmentally friendly way, such as pyrolysis. Pyrolysis
plastic is a process that uses heating and an inert environment to break down the long chains
of polymers that make up plastics into shorter chains [5]. The process can convert plastic
waste into a more useful alternative fuel. This can be done because LDPE plastic is included
in the thermoplastic type, where the basic material comes from petroleum, so it can be
returned to its original form [6].
In the process, pyrolysis can be carried out by adding a catalyst to accelerate the
reaction, lower the reaction temperature, and produce more liquid products and more specific
carbon atoms. Some types of synthetic that are commonly used in the pyrolysis process are
zeolite Y, zeolite A, zeolite X, and Zeolite Socony Mobile-5 (ZSM-5) [7-9]. Of the four
catalysts, the ZSM-5 catalyst is the best catalyst because it produces a higher yield of liquid
products than other catalysts, which is 47.65% [10]. Zeolite Socony Mobile-5 (ZSM-5) is a
type of zeolite with a high Si/Al ratio of 10<Si/Al<∞ [11]. ZSM-5 is a type of zeolite with a
medium pore size (5.1-5.6Å) and a three-dimensional structure limited by 10 ring members.
The advantages of this zeolite are that it can lower the reaction temperature, has high
selectivity and catalytic activity, and has good acid stability. These advantages make ZSM-5
an excellent catalyst for the pyrolysis or cracking process [12]. The complicated synthesis
process involving expensive templates and increasing demand makes the price of ZSM-5
very high. Therefore, an alternative synthesis process for ZSM-5 catalyst is needed, which
has a lower cost and is effective.
ZSM-5 was synthesized by the hydrothermal method by adding silica precursors,
alumina, metal cations and organic templates. The addition of this organic template is done to
facilitate the silica and alumina in forming the ZSM-5 structure. However, organic templates
have disadvantages, namely they are expensive, difficult to degrade, which causes
environmental pollution, and require high temperatures to be released, which causes damage
to the ZSM-5 structure [13]. This is the basis for the development of research on the synthesis
of ZSM-5 without the use of organic templates. Several studies on the synthesis of ZSM-5
without organic templates and using silica precursors that have been conducted are the
synthesis of ZSM-5 from beach sand, natural kaolin, palm fly ash, and rice husk [11, 14-16].
However, these researches still require the addition of expensive seeds and use limited
material supplies, so other alternatives in terms of materials and processes are needed in the
synthesis of ZSM-5 catalysts.
On the other hand, there is a natural disaster that contains abundant silica but has not
been properly utilized, namely Lapindo mud. Based on research conducted by [17], the silica
content in Lapindo mud is 45.3%, which is higher than the silica content in rice husks, which
is only about 18-20%. This silica has the potential to be used as a precursor for the synthesis
of good, abundant and cheap ZSM-5. The purpose of this research is to synthesize ZSM-5
without using an organic template by using silica obtained from Lapindo mud. The resulting
ZSM-5 is used as a catalyst in the pyrolysis process of low-density polyethylene (LDPE)
plastic waste. In addition, pyrolysis was also carried out without the ZSM-5 catalyst. This
was done to determine the effect of adding ZSM-5 catalyst on the yield of liquid products, the
 Malaysian Journal of Chemistry

compounds that make up the liquid products, and the quality of the liquid products from
pyrolysis.

EXPERIMENTAL
Chemicals and Materials
The materials used in this research include Lapindo mud, distilled water, NaOH pa
(Merck), HCl solution pa (Merck), Al(OH)3 pa (Merck), filter paper, and LDPE plastic waste.
Characterization Methods

X-Ray Fluorescence (XRF)

The extracted silica was characterized by XRF to determine the composition of the
elements and oxides in it. The sample was placed on mylar plastic and the surface was
flattened. X-rays were then fired at the sample from below, captured by the detector and
analyzed using MiniPal software. The measurement results obtained were in the form of
percentages of elements and oxides contained in the sample.
X-Ray Diffraction (XRD)
ZSM-5 synthesis results This analyzed using XRD for identification of types phase of
ZSM-5. XRD test was carried out with Cu Κα radiation (λ = 1.5406 Å) at 40 kV and 30 mA,
20 = 10-90° and scan speed 0.02°/sec
Scanning Electron Microscopy (SEM)
The synthesized ZSM-5 was characterized by SEM to analyze the surface topography.
Coated samples with Au-Pd to the entire surface The coated sample is then placed on
instruments and observations were made 50,000 times until the size and ZSM-5 particle
shape clearly.
Fourier Transform Infrared (FTIR)
ZSM-5 was analyzed using FTIR to determine functional groups by mixing KBr
solids and samples with a ratio of 1:10, then shot with infrared light. The data obtained in the
form of an FTIR spectrum was then identified the groups contained therein.
Surface Area by Methylene Blue Adsorption Method
Determination of the surface area of ZSM-5 was carried out using the methylene blue
adsorption method. First, a calibration curve was made by measuring the absorbance of
methylene blue solutions with concentrations of 1, 2, 3, 4, and 5 ppm at a wavelength of 665
nm. The calibration curve was made by plotting the absorbance (y) and concentration (x) of
the standard solution.
Second, the absorbance of ZSM-5 was measured by inserting 0.03 grams of ZSM-5
sample into a beaker glass containing 10 mL of 5 ppm methylene blue solution. The mixture
was stirred for 15 minutes and allowed to stand for 90 minutes. The filtrate was collected and
the absorbance was measured. The absorbance obtained was used to calculate the surface area
using the following formula:
Xm × N × A
S=
M
Where:
S = Surface area (m²/g)
Xm = Mass of methylene blue adsorbed by 1 gram of adsorbent (mg/g)
N = Avogadro's number (6.022 x 1023 particles/mol)
A = Surface area of 1 methylene blue molecule (197.2 x 10-20 m²)
M = Massa molekul metilen biru (320 g/mol)

Gas Chromatography - Mass Spectrometry (GC-MS)

Liquid pyrolysis products diluted 1:10 with n-hexane solvent. The instrument is
programmed between temperatures of 50-260°C with a pressure of 108.2 kPa. The purpose of
this analysis is to determine the structure of the compounds contained in the liquid pyrolysis
products. Measurement results are presented in the form of a graph containing fragment
peaks that can be identified according to the database library.
Extraction of Silica
The Lapindo mud samples has been calcined at a temperature of 900°C and activated
with 2 M HCl, soaked with 2.5 M NaOH at a temperature of 100°C for 4 hours while stirring,
then filtered. The filtrate is added with aquades continued with the addition of 3 M HCl until
pH 7. White precipitate formed, filtered and dried at temperature 100°C until dry.
Synthesis of ZSM-5
The extracted silica is weighed to 2.86 grams, then dissolved in 50 mL 2 M NaOH
and stirred for 30 minutes until homogeneous. Al(OH) 3 is also weighed to 0.8 grams,
dissolved in 14 mL of 7 M NaOH, and refluxed until dissolved. 50 mL of sodium silicate is
mixed with 2.66 mL of sodium aluminate and stirred for 30 minutes, the mixture is incubated
for 24 hours. The mixture is then placed in a reactor and heated at 150°C for 12 hours. The
residue obtained is filtered and washed with distilled water until the pH is neutral, then dried
at room temperature 80°C for 24 hours.
Pyrolysis of LDPE
50 grams of LDPE plastic waste, which has been cleaned and shredded, was fed into
the reactor. ZSM-5 catalyst is added at a ratio of 2.5% (b/b), which was previously heated at
80°C for 30 minutes. The pyrolysis process is carried out at a temperature of 160°C inside the
reactor and 700°C outside the reactor for 6 hours. The pyrolysis was repeated without the
addition of ZSM-5 catalyst. The resulting liquid product is calculated its yield and tested its
quality with some parameters such as density by pycnometer, viscosity by Ostwald
viscometer at the temperature of 40°C, refractive index by refractometer, acid number by
alkalimetric titration and flammability.
RESULTS AND DISCUSSION
Silica Extraction and Characterization
Silica was extracted from samples collected at the Lapindo mud, Porong district,
Sidoarjo regency, 650 meters from the center of the eruption. This sampling was based on
research by [17], who found that the highest silica content was 500-1000 meters from the
center of the eruption. The XRF test results in Table 1 show that the Lapindo mud sample
that had been activated with HCl in this study had a silica content of 58.3%. This content is
higher than the research of [17] which was only 45.3%.
 Malaysian Journal of Chemistry

Table 1. Results of XRF analysis of Lapindo mud and extracted silica

Compound (wt%)
Sample SiO2 Al2O3 Fe2O3 K2O TiO2 Ca Cr2O3 Other
O
Lapindo Mud 58,3 17 14,5 2,84 2,06 1,51 0,063 3,72
Silica 97,7 - 0,624 - 0,12 0,43 0,026 1,1

The extracted silica has a yield of 96.9% with purity reaches 97.7%. This high purity
allows silica extracted from Lapindo mud to be used as a silica precursor in the synthesis of
ZSM-5 [18]. This is because other metal oxides that were previously considered impurities in
silica have been reduced, so they will not interfere with the process of forming the
aluminosilicate structure on the ZSM-5 catalyst.
Synthesis and Characterization of ZSM-5
The zeolite type ZSM-5 in this research was synthesized without using an organic
template with a molar composition of 12Na 2O:100SiO2:2Al2O3:2500H2O. The extracted silica
and aluminum hydroxide were dissolved in NaOH to form sodium silicate and sodium
aluminate. The addition of this NaOH solution acts as a provider of Na + ions which are the
structural directors in the synthesis of this type of zeolite [19]. The formation of the 3D
structure of the aluminosilicate crystals that make up ZSM-5 occurs when the mixture is
heated in an autoclave. The ZSM-5 synthesized in this research has a powder form, white,
and smooth texture.
The success synthesis of ZSM-5 is proven by the results of the XRD characterization
research peaks. The diffractogram of ZSM-5 from the synthesis in Figure l(a) has a similar
value of 2θ and d-spacing with the ZSM-5 standard in JCPDS No. 10 235-242 [11]. The
diffractogram also shows a typical peak of ZSM-5, at 2θ = 24.41° which shows the
diffraction pattern of the MFI crystal structure [20]. The sharp peaks produced indicate that
the synthesized ZSM-5 has a crystalline phase with a crystallinity level of 71.7%, higher than
ZSM-5 in the research of [21] which used silica precursors from rice husks with a
crystallinity of 54.42%. High crystallinity correlates with the regularity of the structure and
pore size of the synthesized ZSM-5.
ZSM-5 synthesized from Lapindo mud silica was also characterized by SEM to
determine its surface morphology. The SEM characterization results in Figure 1(b) show that
the particle size distribution of ZSM-5 is uniform. This supports the XRD characterization
results that ZSM-5 is in a crystalline phase. The SEM results also show a hexagonal geometry
which is a typical geometry of ZSM-5 [21-22]

(b)
 (a)

Figure 1. (a) ZSM-5 diffractogram (b) Morphology of ZSM-5 at 50.000x

The results of FTIR characterization also confirm the success of ZSM-5 synthesis in
this research. Figure 2 shows that the resulting spectrum shows the vibrational bands of
functional groups of ZSM-5 with certain wavenumbers, such as 1103.28 cm -1 and 981.77 cm-1
which are asymmetric stretching vibrations T-O-T (T = Si, Al); 759.95 cm -1 which is a
symmetric stretching vibration T-O-T (T = Si, Al); 574.79 cm -1 and 621 cm-1 which are
double ring vibrations in the pentasil group of ZSM-5; and 499.56 cm -1 which is a bending
vibration of T-O-T (T = Si, Al). Thus, it can be said that ZSM-5 was successfully synthesized
using silica precursors extracted from Lapindo mud

Figure 2. Spectra FTIR of ZSM-5 Synthesized

ZSM-5 was used in this research as a catalyst in the pyrolysis process, so surface area
analysis is necessary to be carried out. The surface area of the ZSM-5 catalyst analyzed using
the adsorption method methylene blue measured at length 665 nm wave. Calculation results
show that the surface area ZSM-5 in this research was 283.94 m²/g, the surface area is close
to ZSM-5 commercially, namely ~300 m²/g [23]. The size of this surface area allows the
distribution of acid sites on ZSM-5 is more even, so the site active for the polymer cracking
process more LDPE plastic.
Pyrolysis of LDPE Plastic Waste
The products produced from the pyrolysis process are divided into three phases,
namely gas, solid (coke), and liquid. However, the main focus of this research is the liquid
product, while the gas and coke products are not calculated for their yield. The liquid product
produced from the LDPE plastic pyrolysis process with the addition of ZSM-5 catalyst has a
difference compared to without the addition of ZSM-5 catalyst. The difference shown is in
the amount of yield, where with the addition of the catalyst the yield produced is 35.3%,
while without the addition of the catalyst the yield produced is only 13.8%. Another
difference is in the initial temperature of the dripping liquid. The addition of ZSM-5 catalyst
reduces the temperature by 10°C as shown in Table 2. This indicates that the addition of
ZSM-5 catalyst to the pyrolysis process can increase the yield of the liquid product produced
while reducing the reaction temperature during the pyrolysis process [5].

Table 2. Difference of Using ZSM-5 on Yield and Temperature

Sampel Yield First Temperature of Liquid Drip
 Malaysian Journal of Chemistry

0% ZSM-5 13,8% 52°C

2,5% ZSM-5 35,3% 42°C

The quality of the liquid products from pyrolysis was tested using several parameters
to determine the type of fuel oil produced. Based on the data in Table 3, it can be seen that
both liquid products are similar to gasoline fuel in terms of density, viscosity, and refractive
index. This is because the temperature used during the pyrolysis process in this study was
limited to 160°C. This temperature is the temperature range at which the compounds that
make up gasoline can evaporate [24]. However, the liquid product produced with the ZSM-5
catalyst has a lower acid number and is within the SNI gasoline range (SNI 8415:2017)
compared to without the catalyst, so it can be said that the liquid product produced with the
ZSM-5 catalyst has a better quality.

Table 3. Quality of Pyrolisis Liquid Product

Sample Density Viskocity Refractive Acid Number Flame
(g/mL) (cSt) Index (mg KOH/g) Colour
0% ZSM-5 0,761 0,69 1,422 2,24 Yellow
2,5% ZSM-5 0,756 0,64 1,423 0,278 Yellow
Standart of 0,710-0770 0,65 1,407-1,446 0,2-0,5 -
Gasoline

Liquid products from pyrolysis also analyzed using GC-MS for knowing the
compatibility of chemical compounds compiler with quality analysis results that has been
done previously. Based on Table 4 shows that the liquid product consists of straight-chain
alkanes and alkenes or branched with a range of C 8-C12. These compounds enter into the
range of constituent hydrocarbons gasoline C5-C12, until the result quality analysis and GC-
MS data have compatibility. The percentage of the number of compounds with C 8-C12 chain
using a catalyst ZSM-5 is higher than without catalyst. This can happen because the ZSM-5
catalyst shows good selectivity for compounds with these chains, which is also supported by
the research results of [5], which showed the same thing. In addition, the two largest
compound contents (13.26%) in liquid products using the ZSM-5 catalyst are branched chain
alkanes, namely 3,5-dimethyloctane and 2,4-dimethylhexane. The presence of these
branched-chain alkanes provides better fuel quality than straight-chain alkanes and alkenes
because branched-chain alkanes do not readily undergo spontaneous combustion in the
engine, so the resulting engine knock is less [25].

Table 4. Compound of Pyrolisis Liquid Product

Chemical Percentage (%)
Chemical Name
Compound 2,5% ZSM-5 0% ZSM-5
C10H22 3,5-dimethyloctane 6,78 5,19
C8H18 2,4-dimethylhexane 6,48 5,54
C9H20 Nonane 6,01 5,10
C11H24 Undecane 5,36 6,37
C10H20 2-decene 4,31 0,87
C10H20 1-decene 4,21 5,90
C9H18 1-nonene 4,06 4,96
 C10H20 1-undecene 3,84 5,59
C8H16 1-octene 3,71 5,11
C10H20 5-undecene 3,28 -
C12H26 Dodekane 3,09 5,01
C12H24 1-dodekene 1,85 -
C9H18 2-nonene 1,83 -
Total Area 54,81 49,64

CONCLUSION

ZSM-5 has been successfully synthesized in this research using silica precursor from
Lapindo mud. The success of ZSM-5 synthesis is supported by the results of XRD, SEM, and
FTIR characterization which show peaks, geometry, and vibration bands typical of ZSM-5.
The surface area of ZSM-5 in this research is 283.94 m²/g, so that the distribution of active
sites for pyrolysis reactions is greater. The yield of liquid pyrolysis products produced with
the addition of ZSM-5 catalyst increased by 35.3% compared to without using ZSM-5
catalyst which was only 13.8%. Liquid products from pyrolysis using ZSM-5 catalyst have
density, viscosity, refractive index, flame color, and acid number values that fall within the
SNI range for gasoline fuel (SNI 8415:2017). In addition, the chemical compounds that make
up the two liquid pyrolysis products are dominated by C 8-C12 with the two largest
components in the liquid product using the ZSM-5 catalyst in the form of branched chains
which are better used in fuel.

ACKNOWLEDGEMENTS

All authors would like to thank the Ministry of Education, Culture, Research, and
Technology Indonesia and Universitas Negeri Malang for providing financial support for this
research through the Student Creativity Program - Exact Research 2024.

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